CN109678213A - A kind of recycling and reuse method of lithium-ion battery lithium iron phosphate waste material - Google Patents
A kind of recycling and reuse method of lithium-ion battery lithium iron phosphate waste material Download PDFInfo
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- CN109678213A CN109678213A CN201811601133.9A CN201811601133A CN109678213A CN 109678213 A CN109678213 A CN 109678213A CN 201811601133 A CN201811601133 A CN 201811601133A CN 109678213 A CN109678213 A CN 109678213A
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- Prior art keywords
- lithium
- ion battery
- recycling
- waste material
- iron phosphate
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G49/00—Compounds of iron
- C01G49/12—Sulfides
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B32/00—Carbon; Compounds thereof
- C01B32/05—Preparation or purification of carbon not covered by groups C01B32/15, C01B32/20, C01B32/25, C01B32/30
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M10/00—Secondary cells; Manufacture thereof
- H01M10/54—Reclaiming serviceable parts of waste accumulators
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/36—Selection of substances as active materials, active masses, active liquids
- H01M4/58—Selection of substances as active materials, active masses, active liquids of inorganic compounds other than oxides or hydroxides, e.g. sulfides, selenides, tellurides, halogenides or LiCoFy; of polyanionic structures, e.g. phosphates, silicates or borates
- H01M4/581—Chalcogenides or intercalation compounds thereof
- H01M4/5815—Sulfides
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/36—Selection of substances as active materials, active masses, active liquids
- H01M4/58—Selection of substances as active materials, active masses, active liquids of inorganic compounds other than oxides or hydroxides, e.g. sulfides, selenides, tellurides, halogenides or LiCoFy; of polyanionic structures, e.g. phosphates, silicates or borates
- H01M4/583—Carbonaceous material, e.g. graphite-intercalation compounds or CFx
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/40—Electric properties
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/10—Energy storage using batteries
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02W—CLIMATE CHANGE MITIGATION TECHNOLOGIES RELATED TO WASTEWATER TREATMENT OR WASTE MANAGEMENT
- Y02W30/00—Technologies for solid waste management
- Y02W30/50—Reuse, recycling or recovery technologies
- Y02W30/84—Recycling of batteries or fuel cells
Abstract
The invention discloses a kind of recycling and reuse methods of lithium-ion battery lithium iron phosphate waste material.Method includes the following steps: carrying out acidleach to it for after LiFePO4 waste recovery, obtained leachate and sulfide are subjected to hydro-thermal reaction, obtain iron-sulphide particles；Carbon heat reducing is carried out to iron sulfide later, obtains carbon coating ferrous sulfide composite material.The composite material may be used as anode material for lithium-ion batteries, have preferable storage lithium performance.This method will be worth lower LiFePO4 of scrapping and be converted into the higher material of value, promote material recovery value.And this method rate of recovery is higher, can achieve 90% or more to the rate of recovery of ferro element, and the rate of recovery of subsequent elemental lithium also can reach 90% or more.
Description
Technical field
The invention belongs to lithium ion battery recycling fields, and in particular to a kind of recycling of lithium-ion battery lithium iron phosphate waste material
And reuse method.
Background technique
With the increase of social development and electric car usage amount, the quantity of waste battery is also steeply risen.These are scrapped
Battery not only results in serious environmental pollution and heavy metal pollution, serious harm can be also brought to human health if do not handled.
LiFePO4 is a kind of anode material for lithium-ion batteries favored by batteries of electric automobile, has olivine knot
Structure, in this configuration, iron atom and the close bonding of oxygen atom are constituted octahedra；Lithium atom and the close bonding of oxygen atom constitute eight
Furthermore face body adds phosphate radical tetrahedron again.It is tightly combined between atom in LiFePO4, so that material safety is very high.?
In the batteries of electric automobile scrapped, some uses lithium iron phosphate positive material, and learies are very big.
Traditional ferric phosphate lithium cell waste material recovery method, which is concentrated mainly on, decomposes material, single-element recycling.
It is well known that ferro element is inexpensive, if LiFePO4 recycled in the form of ferro element, recovery value is very low.
Also method proposes that carrying out high temperature solid-state to LiFePO4 waste material directly repairs, and is allowed to performance and is regenerated, but due in waste material
Acetylene black and high-temperature process after bonding agent decompose generate impurity can to material regeneration generate side reaction.In view of impurity member
Element and LiFePO 4 material itself are to the rigors of preparation condition, so promotion degree of this kind of method to material property
It is very limited.
Summary of the invention
In view of the shortcomings of the prior art and shortcoming, the primary purpose of the present invention is that providing a kind of lithium ion battery phosphorus
The recycling and reuse method of sour iron lithium waste material.It is after leaching LiFePO 4 material in this method, ferro element therein is straight
It connects and is prepared into lithium ion battery ferrous sulfide, elemental lithium therein is then recycled in the form of lithium carbonate, greatly promotes its time
Receive value.
The object of the invention is achieved through the following technical solutions:
A kind of recycling and reuse method of lithium-ion battery lithium iron phosphate waste material, comprising the following steps:
(1) waste and old lithium ion battery is disassembled, separates anode pole piece；Obtained anode pole piece is soaked in organic molten
In agent, binder is dissolved, positive active material is separated with aluminium flake, obtains LiFePO4；
(2) obtained LiFePO4 is subjected to acidleach, is allowed to dissolve, then filter, obtains filtrate；
(3) it with the constituent content in ICP (inductively coupled plasma atomic emission spectrometer) detection filtrate, is filtering later
Sulphur source is added in liquid, obtained mixture is transferred in water heating kettle and carries out hydro-thermal reaction, the product that hydro-thermal reaction obtains is
Fe2S3, product Fe is collected after cooling respectively2S3With hydro-thermal reaction filtrate；
(4) using ICP detection hydro-thermal reaction filtrate in Li content, backward hydro-thermal reaction filtrate in appropriate carbonic acid is added
Sodium, adjusting filtrate pH value is 7~10, and stirring is allowed to precipitate, and obtains Li2CO3；
(5) Fe that will be obtained2S3It is mixed with reproducibility containing carbon matrix precursor, is sintered in protective atmosphere later, obtains carbon coating
FeS2(FeS2/C)。
Soaking temperature described in step (1) controls between 30~70 DEG C, and soaking time is 3~10h.
Step (1) organic solvent is N-Methyl pyrrolidone (NMP) and/or N,N-dimethylformamide (DMF).
The acid solution that acidleach described in step (2) uses is the combination of inorganic acid and hydrogen peroxide or organic acid and mistake
The combination of hydrogen oxide.
Sour (inorganic acid or organic acid) concentration control is in 0.8~2mol/L in the acid solution, and concentration of hydrogen peroxide is 5%~
15% (volume).
The inorganic acid is one or more of sulfuric acid, nitric acid and hydrochloric acid, and the organic acid is oxalic acid and/or lemon
Lemon acid.
Acidleach temperature described in step (2) controls between 50~90 DEG C, and time control exists in 3~10h, solid-to-liquid ratio control
10~20g/L.
Sulphur source described in step (3) includes (NH4)2S, one or more of urea and thiocarbamide, sulphur source according to mole
Than controlling additional amount for the ratio of Fe:S=1:1.5~3 (preferably 1:1.5~2).
Hydrothermal temperature described in step (3) is 150~200 DEG C, and the time is 5~15h, preferably anti-at 180~200 DEG C
Answer 5~8h.
Suitable organic solvent can be added in step (3) in water heating kettle and carry out hydro-thermal reaction together with mixture, control
The pattern and crystal orientation of final product processed.
The organic solvent includes one or more of ethyl alcohol, methanol and polyethylene glycol；The addition of organic solvent
Amount is the 1%~10% of filtrate volume.
Sodium carbonate controls additional amount according to the ratio that molar ratio is Li:Na=1:1~1.1 in step (4).
Li obtained in step (4)2CO3It is further commercially available after purification.
Reproducibility described in step (5) includes one of citric acid, glucose and ascorbic acid or two containing carbon matrix precursor
Kind or more；The Fe2S3It is 1:1~3, preferably 1:1~1.5 with mass ratio containing carbon matrix precursor.
Described in step (5) sintering refer in 600~900 DEG C of 6~10h of sintering, preferably 700~800 DEG C sintering 8~
9h。
Protective atmosphere described in step (5) is nitrogen or inert gas.
Compared with prior art, the present invention has the following advantages and beneficial effects:
The method of the present invention sufficiently can convert Fe for the iron in LiFePO42S3, and through the primary direct shape of carbothermic method
At carbon encapsulated material FeS2/ C promotes materials conductive rate.This method will be worth it is lower scrap LiFePO4 be converted into value compared with
High material promotes material recovery value.And this method rate of recovery is higher, to the rate of recovery of ferro element can achieve 90% with
On, and the rate of recovery of subsequent elemental lithium also can reach 90% or more.Obtained material charging and discharging capacity with higher, and follow
Ring performance is preferable, can be directly used in lithium ion battery.
Detailed description of the invention
Fig. 1 is anode material for lithium-ion batteries FeS prepared by embodiment 12The cycle performance test chart of/C.
Specific embodiment
Below with reference to embodiment and attached drawing, the present invention is described in further detail, but embodiments of the present invention are unlimited
In this.
Embodiment 1
(1) waste and old lithium ion battery is disassembled, separates anode pole piece；Obtained anode pole piece is soaked in N- methyl
In pyrrolidones (NMP), binder is dissolved, positive active material is separated with aluminium flake, obtains LiFePO4；Soaking temperature is 50
DEG C, soaking time 5h.
(2) obtained LiFePO4 is subjected to acidleach, is allowed to dissolve, then filters, remove filter residue, obtain clarification leachate
(i.e. filtrate)；The acid solution that acidleach uses is sulfuric acid+hydrogenperoxide steam generator, and sulfuric acid concentration is 1.5mol/L, hydrogen peroxide in acid solution
Concentration is 10%；In acidleach, solid-to-liquid ratio 10g/L, temperature is 60 DEG C, reaction time 5h.
(3) with the constituent content in ICP detection filtrate, sulphur source (NH is added in filtrate later4)2(Fe:S molar ratio is S
1:1.5), obtained mixture is transferred in water heating kettle, the hydro-thermal reaction 8h at 180 DEG C；The product that hydro-thermal reaction obtains is i.e.
For Fe2S3, product Fe is collected after cooling respectively2S3With hydro-thermal reaction filtrate；
(4) using ICP detection hydro-thermal reaction filtrate in Li content, backward hydro-thermal reaction filtrate in sodium carbonate is added
(Li:Na molar ratio is 1:1), adjusting filtrate pH value is 7.5, stirs to get white precipitate Li2CO3, it is carried out further net
Change, obtains commercial Li2CO3；
(5) Fe that will be obtained2S3It is mixed with citric acid with mass ratio 1:1, later at 700 DEG C, inert atmosphere protection sintering
9h obtains anode material for lithium-ion batteries FeS2/C。
To anode material for lithium-ion batteries FeS obtained2/ C carries out cycle performance test, and test result is shown in Fig. 1.From figure
It can be seen that current density is 0.5A g in voltage range between 0.05~3V-1When, first discharge specific capacity 638.9mAh
G-1, specific discharge capacity still reaches 500.5mAh g-1 after 50 circulations, and capacity retention ratio 78.3% is shown good
Cycle performance.
It is 95.6% to the rate of recovery of elemental lithium in the present embodiment, the rate of recovery to ferro element is 97.1% through detecting.
Embodiment 2
(1) waste and old lithium ion battery is disassembled, separates anode pole piece；Obtained anode pole piece is soaked in N- methyl
In pyrrolidones (NMP), binder is dissolved, positive active material is separated with aluminium flake, obtains LiFePO4；Soaking temperature is 60
DEG C, soaking time 4h.
(2) obtained LiFePO4 is subjected to acidleach, is allowed to dissolve, then filters, remove filter residue, obtain clarification leachate
(i.e. filtrate)；The acid solution that acidleach uses is sulfuric acid+hydrogenperoxide steam generator, and sulfuric acid concentration is 1.7mol/L, hydrogen peroxide in acid solution
Concentration is 8%；In acidleach, solid-to-liquid ratio 15g/L, temperature is 60 DEG C, reaction time 4h.
(3) with the constituent content in ICP detection filtrate, sulphur source (NH is added in filtrate later4)2(Fe:S molar ratio is S
1:1.8), and the ethyl alcohol that volume is leachate volume 5% is added, obtained mixture is transferred in water heating kettle later, 190
Hydro-thermal reaction 6h at DEG C；The product that hydro-thermal reaction obtains is Fe2S3, product Fe is collected after cooling respectively2S3It is filtered with hydro-thermal reaction
Liquid；
(4) using ICP detection hydro-thermal reaction filtrate in Li content, backward hydro-thermal reaction filtrate in sodium carbonate is added
(Li:Na molar ratio is 1:1.05), adjusting filtrate pH value is 8, stirs to get white precipitate Li2CO3, it is carried out further net
Change, obtains commercial Li2CO3；
(5) Fe that will be obtained2S3It is mixed with citric acid with mass ratio 1:1.5, later at 800 DEG C, inert atmosphere protection is burnt
8h is tied, anode material for lithium-ion batteries FeS is obtained2/C。
It is 93.4% to the rate of recovery of elemental lithium in the present embodiment, the rate of recovery to ferro element is 96.5% through detecting.
The above embodiment is a preferred embodiment of the present invention, but embodiments of the present invention are not by above-described embodiment
Limitation, other any changes, modifications, substitutions, combinations, simplifications made without departing from the spirit and principles of the present invention,
It should be equivalent substitute mode, be included within the scope of the present invention.
Claims (10)
1. a kind of recycling and reuse method of lithium-ion battery lithium iron phosphate waste material, which comprises the following steps:
(1) waste and old lithium ion battery is disassembled, separates anode pole piece；Obtained anode pole piece is soaked in organic solvent
In, binder is dissolved, positive active material is separated with aluminium flake, obtains LiFePO4；
(2) obtained LiFePO4 is subjected to acidleach, is allowed to dissolve, then filter, obtains filtrate；
(3) with the constituent content in ICP detection filtrate, sulphur source is added in filtrate later, obtained mixture is transferred to water
Hydro-thermal reaction is carried out in hot kettle, the product that hydro-thermal reaction obtains is Fe2S3, product Fe is collected after cooling respectively2S3It is anti-with hydro-thermal
Answer filtrate；
(4) using ICP detection hydro-thermal reaction filtrate in Li content, backward hydro-thermal reaction filtrate in sodium carbonate is added, adjusting
Filtrate pH value is 7~10, and stirring is allowed to precipitate, and obtains Li2CO3；
(5) Fe that will be obtained2S3It is mixed with reproducibility containing carbon matrix precursor, is sintered, obtains carbon-coated in protective atmosphere later
FeS2。
2. the recycling and reuse method of lithium-ion battery lithium iron phosphate waste material according to claim 1, which is characterized in that
Soaking temperature described in step (1) controls between 30~70 DEG C, and soaking time is 3~10h；
Step (1) organic solvent is N-Methyl pyrrolidone and/or N,N-dimethylformamide.
3. the recycling and reuse method of lithium-ion battery lithium iron phosphate waste material according to claim 1, which is characterized in that
The acid solution that acidleach described in step (2) uses is combination or organic acid and the hydrogen peroxide of inorganic acid and hydrogen peroxide
Combination；
The concentration of inorganic acid or organic acid is 0.8~2mol/L in acid solution, and concentration of hydrogen peroxide is 5%~15% (volume).
4. the recycling and reuse method of lithium-ion battery lithium iron phosphate waste material according to claim 1, which is characterized in that
Acidleach temperature described in step (2) controls between 50~90 DEG C, and time control is controlled in 3~10h, solid-to-liquid ratio in 10~20g/
L。
5. the recycling and reuse method of lithium-ion battery lithium iron phosphate waste material according to claim 1, which is characterized in that
Sulphur source described in step (3) includes (NH4)2S, one or more of urea and thiocarbamide；Sulphur source is Fe:S according to molar ratio
The ratio of=1:1.5~3 controls additional amount.
6. the recycling and reuse method of lithium-ion battery lithium iron phosphate waste material according to claim 1, which is characterized in that
Hydrothermal temperature described in step (3) is 150~200 DEG C, and the time is 5~15h.
7. the recycling and reuse method of lithium-ion battery lithium iron phosphate waste material according to claim 1, which is characterized in that
Suitable organic solvent is added in water heating kettle in step (3) and carries out hydro-thermal reaction together with mixture, controls final product
Pattern and crystal orientation；The organic solvent includes one or more of ethyl alcohol, methanol and polyethylene glycol；Organic solvent
Additional amount be filtrate volume 1%~10%.
8. the recycling and reuse method of lithium-ion battery lithium iron phosphate waste material according to claim 1, which is characterized in that
Sodium carbonate controls additional amount according to the ratio that molar ratio is Li:Na=1:1~1.1 in step (4).
9. the recycling and reuse method of lithium-ion battery lithium iron phosphate waste material according to claim 1, which is characterized in that
Reproducibility described in step (5) includes one or more of citric acid, glucose and ascorbic acid containing carbon matrix precursor；Institute
State Fe2S3It is 1:1~1:3 with mass ratio containing carbon matrix precursor.
10. the recycling and reuse method of lithium-ion battery lithium iron phosphate waste material according to claim 1, feature exist
In sintering described in step (5) refers in 600~900 DEG C of 6~10h of sintering.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201811601133.9A CN109678213A (en) | 2018-12-26 | 2018-12-26 | A kind of recycling and reuse method of lithium-ion battery lithium iron phosphate waste material |
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| CN201811601133.9A CN109678213A (en) | 2018-12-26 | 2018-12-26 | A kind of recycling and reuse method of lithium-ion battery lithium iron phosphate waste material |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110620278A (en) * | 2019-09-25 | 2019-12-27 | 深圳清华大学研究院 | Method for recovering anode material of waste lithium iron phosphate battery |
| CN110690429A (en) * | 2019-10-14 | 2020-01-14 | 王敏 | Treatment method of waste lithium iron phosphate |
| CN115312903A (en) * | 2022-10-12 | 2022-11-08 | 常州锂源新能源科技有限公司 | Method for preparing rate type lithium iron phosphate by regenerating waste lithium iron phosphate |
| JP7286085B2 (en) | 2019-07-16 | 2023-06-05 | 太平洋セメント株式会社 | Method for recovering lithium from lithium-ion batteries |
-
2018
- 2018-12-26 CN CN201811601133.9A patent/CN109678213A/en active Pending
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP7286085B2 (en) | 2019-07-16 | 2023-06-05 | 太平洋セメント株式会社 | Method for recovering lithium from lithium-ion batteries |
| CN110620278A (en) * | 2019-09-25 | 2019-12-27 | 深圳清华大学研究院 | Method for recovering anode material of waste lithium iron phosphate battery |
| CN110690429A (en) * | 2019-10-14 | 2020-01-14 | 王敏 | Treatment method of waste lithium iron phosphate |
| CN115312903A (en) * | 2022-10-12 | 2022-11-08 | 常州锂源新能源科技有限公司 | Method for preparing rate type lithium iron phosphate by regenerating waste lithium iron phosphate |
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Application publication date: 20190426 |